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  • supercritical fluid chromatography  (9)
  • PLOT column  (2)
  • Biochemistry and Biotechnology  (1)
  • 1
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 3 (1991), S. 229-239 
    ISSN: 1040-7685
    Keywords: sample introduction ; injection ; supercritical fluid chromatography ; open tubular columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: As in the case of all chromatographic methods, the ideal sample introduction method for supercritical fluid chromatography (SFC) would provide a narrow and sharp solvent peak (or no solvent peak), quantitative transfer of the sample into the column, and high reproducibility. Elimination of the solvent before the solutes enter the column would be preferred; however, this practice is always associated with the risk of partial solute elimination. In open tubular column SFC, samples are normally introduced using a smallvolume internal loop valve. These valves can be operated such that none, some, or all of the solvent is eliminated. Several approaches were quantitatively evaluted, and optimized conditions were determined. Particular attention was given to trace analysis. The minimum detectable levels (S/N 〉4) achievable using a flame ionization detector were determined to be approximately 30 ng (150 ppm) for split injection, 4 ng (20 ppm) for delayed split injection, and 1 ng (5 ppm) for direct injection.
    Additional Material: 8 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 7 (1995), S. 207-212 
    ISSN: 1040-7685
    Keywords: charcoal ; active carbon ; PLOT column ; column technology ; gas chromatography ; permanent gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of charcoal porous layer open tabular (PLOT) columns, and their application to the separation of permanent gases and light hydrocarbons are reported. Two types of charcoal, coconut and darco charcoal, were used to prepare columns from fused silica capillaries. The performance of these columns was compared to that of a commercially available carbon molecular sieve PLOT column. The coconut charcoal PLOT column produced good retention and resolution for both permanent gases and light hydrocarbons; all separations were achieved in less than eight minutes under isothermal conditions. © 1995 John Wiley & Sons, Inc.
    Additional Material: 9 Ill.
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  • 3
    ISSN: 1040-7685
    Keywords: multidimensional ; supercritical fluid chromatography ; liquid crystal polysiloxane ; polycyclic aromatic hydrocarbons ; coal tar ; petroleum distillate ; carbofuran ; capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A multidimensional system based on capillary supercritical fluid chromatography (SFC) was constructed that utilizes a simple flow-switching interface between two open-tubular 50-μm i.d. columns. A novel solvent-venting injection technique was incorporated in the system that enables single or multiple 0.5-μL volumes to be injected into an uncoated, yet deactivated, length of capillary precolumn without flooding of the analytical column. The effectiveness of multidimensional capillary SFC (SFC-SFC) for complex mixtures is demonstrated by the analysis of polycyclic aromatic hydrocarbons (PAH) in a coal tar extract, the trace determination of a methylcarbamate pesticide and its metabolites in a bird extract, and a group-type separation of hydrocarbons in a high-boiling petroleum distillate. These examples show for the first time that capillary SFC-SFC is a complementary alternative to other multidimensional chromatographic methods involving liquid or gaseous mobile phases.
    Additional Material: 12 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 1 (1989), S. 207-211 
    ISSN: 1040-7685
    Keywords: supersonic jet spectroscopy ; supercritical fluid chromatography ; sheath-flow nozzle ; capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Supersonic jet spectroscopic detection has been successfully coupled to capillary supercritical fluid chromatography by introduction of the supercritical effluent into a secondary flow of argon, before supersonic expansion of the combined flow through a converging nozzle. At pressures of 6-10 atm, the flowing sheath of argon efficiently carries eluting sample through a 25-p.m nozzle orifice into the supersonic jet. Dead volumes are negligible in this arrangement, and high-resolution fluorescence excitation spectra are obtained. Perylene and benzo[a]pyrene were selectively detected in a standard reference coal tar sample at detection limits of 150 pg and 5 ng, respectively.
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 3 (1991), S. 521-529 
    ISSN: 1040-7685
    Keywords: solvent vent ; large volume injection ; open tubular columns ; supercritical fluid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of small internal diameter precolumns (11-25-μm i. d.) helped solute focussing when using solvent vent sample introduction in open tubular column supercritical fluid chromatography (SFC). Column efficiencies were similar to those obtained with split injection (3000-5000 plates m-1). Trace analysis in SFC was improved because large volumes (1 μL) could be introduced for analysis with little sacrifice in column efficiency.
    Additional Material: 11 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 7 (1995), S. 153-158 
    ISSN: 1040-7685
    Keywords: silica gel ; PLOT column ; column technology ; gas chromatography ; light hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We report a simple method for the preparation of silica PLOT columns using fused silica capillaries. In this method, silica particles were suspended in a methylene chloride/pentane solution containing polymethylhydrosiloxane and passed through the capillary tubing. This caused the silica particles to be dynamically coated on the inner wall of the fused silica capillary. The column was dried and heated, which facilitated the simultaneous deactivation and bonding of a uniform mono-layer of porous silica on the inner wall of the capillary tubing. These columns were used to separate light hydrocarbons, chlorinated hydrocarbons, and aromatic compounds.
    Additional Material: 6 Ill.
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  • 7
    ISSN: 1040-7685
    Keywords: supercritical fluid chromatography ; mass spectrometry ; negative ion ; chemical ionization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of mass spectrometry in the negative ion mode with capillary column supercritical fluid chromatography is described. The supercritical fluid chromatography mobile phase (CO2) was used as the primary reagent gas to generate thermalized electrons and reagent anions (such as O- and CO2-). When trace amounts of CH4 or NH3 gas were also introduced into the chemical ionization source, the mass spectrometer sensitivity was increased. Detection limits (S/N = 5) for heptachlor were determined to be 20 pg and 200 fg for full scan and selected ion monitoring modes, respectively. Mass spectra of a cyclic peptide, valinomycin, obtained with these mixed reagents (CH4 + CO2 and NH3 + CO2) gave the molecular anion at m/z 1110 as the most abundant ion and additional fragment ions that yielded peptide sequence information.
    Additional Material: 9 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 495-501 
    ISSN: 1040-7685
    Keywords: supercritical fluid chromatography ; open tubular columns ; electrochemical detection ; platinum microelectrode ; water modified carbon dioxide ; ferrocene derivatives ; diphenylamine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A miniaturized electrochemical detector for microcolumn separations has been developed. The detector was used in open tubular column supercritical fluid chromatography (SFC) with a mobile phase consisting of supercritical carbon dioxide with water below saturation. The detector is compatible with pressure programmed conditions, as is illustrated by the separation of ferrocene, acetylferrocene, and benzoylferrocene.
    Additional Material: 5 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 385-393 
    ISSN: 1040-7685
    Keywords: supercritical fluid extraction ; supercritical fluid chromatography ; solid phase adsorption ; on-line ; sample introduction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated setup for on-line solid phase adsorption (SPA)/supercritical fluid extraction (SFE)/supercritical fluid chromatography (SFC) was evaluated. Low nanogram amounts of analytes dissolved in ethanol were delivered in the form of injections (≥ 10 μL) to the solid phase adsorbent consisting of deactivated glass beads, and the analytes were then extracted with supercritical carbon dioxide. The analytes were applied to the adsorbent by an autosampler, which also controlled rinsing and adsorption times. During the chromatographic run, the adsorbent was automatically cleaned with high density supercritical carbon dioxide to be ready for the subsequent injection. Memory effects were between 0 and 4% depending on the analyte, and the reproducibilities were between 6 and 17% of the relative peak areas.
    Additional Material: 3 Ill.
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  • 10
    ISSN: 1040-7685
    Keywords: stationary phase ; liquid crystal polysiloxane ; supercritical fluid chromatography ; capillary column ; steroids ; androstanes ; estrogens ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A liquid crystalline biphenylcarboxylate ester polysiloxane stationary phase was used to study the effect of solute structure on retention for the separation of isomeric steroids in capillary supercritical fluid chromatography. It was determined that theretention mechanism is related to solute molecular shape rather than to properties such as volatility or polarity. The elution order of isomeric androstanes and estrogens could be correlated with the planarity of molecules: more-planar molecules were retained longer on the column. The resolution of steroid isomers was improved significantly using the liquid crystalline stationary phase when compared with results obtained using other stationary phases.
    Additional Material: 6 Ill.
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